三甲基硅重氮甲烷衍生化-气相色谱法测定水果蔬菜中乙烯利的残留 |
投稿时间:2018-04-14
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引用本文:陈克云,王艳丽,沈祥震,等.三甲基硅重氮甲烷衍生化-气相色谱法测定水果蔬菜中乙烯利的残留[J].农药学学报,2018,20(4):495-499. |
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中文摘要:针对水果蔬菜中乙烯利的残留,建立了三甲基硅重氮甲烷衍生化-气相色谱的分析方法。样品用V(甲醇):V(盐酸)=9:1的溶液提取,无水乙醚萃取,三甲基硅重氮甲烷衍生化15 min,采用气相色谱-质谱法定性,气相色谱仪-火焰光度检测器(GC-FPD)检测,外标法定量。结果显示:在0.01~2 mg/L范围内,乙烯利的质量浓度与其对应的峰面积间线性关系良好,相关系数大于0.999 6;此方法检出限为0.01 mg/kg,定量限为0.03 mg/kg;在辣椒、番茄、香蕉、苹果和梨的空白果蔬样品中分别添加0.01、0.1和1 mg/kg 3个水平下,回收率为93%~102%,相对标准偏差为4.2%~7.3%。该方法准确度和灵敏度高,抗干扰能力强,能准确并快速测定出水果、蔬菜中乙烯利的残留量。 |
中文关键词:三甲基硅重氮甲烷 衍生化 气相色谱 水果 蔬菜 乙烯利 残留 |
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Determination of ethephon residue in fruits and vegetables by gas chromatography after derivatization with (trimethylsilyl)diazomethane |
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Abstract:An analytical method for the determination of ethephon residue in fruits and vegetables was established by using gas chromatography after derivatization with (trimethylsilyl)diazomethane. The samples were extracted with a mixture of hydrochloric acid and methanol (9:1, V/V). It was then extracted with anhydrous ether and subjected to derivatization by (trimethylsilyl)diazomethane. The extracts were determined by gas chromatography with the external standard method and qualitative by gas chromatography-mass spectrometry. The calibration curve of ethephon residue was linear in the range of 0.01-2 mg/L with correlation coefficients higher than 0.999 6. The detection limit of this method was 0.01 mg/kg and the limit of quantification was 0.03 mg/kg. In the samples of fruits and vegetables at spiked levels from 0.01 mg/kg to 1mg/kg, the recovery was 93%-102% with the relative standard deviation from 4.2%-7.3%. The method has the advantages of high accuracy, good sensitivity, and strong anti-interference ability, which can be used for the accurate and rapid determination of ethephon residues in fruits and vegetables. |
Key words:(trimethylsilyl)diazomethane derivatization gas chromatography fruit vegetable ethephon residue |
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